Processes of reclaiming rubber and reclaimed rubber products



Sept. 29, 1953 J. c. ELGIN ETAL 2,653,915

PROCESSES OF RECLAIMING RUBBER. AND

RECLAIMED RUBBER PRODUCTS Filed Feb. 3, 1951 ZSheets-Sheet I Foecw PLnsncarmG Fozcme I FOECING W 7 2 IN V EN TOR. Jossru Chrron EL 6m! E nw/mo 5' Snack Sept. 29, 1953 J. c. ELGIN ETAL 2,653,915

. PROCESSES OF RECLAIMING RUBBER, AND

RECLAIMED RUBBER PRODUCTS Filed Feb. 3, 1951 Sheets-Sheet 2 Patented Sept. 29, 1953 PROCESSES OF RECLAIMING RUBBER AND RECLAIMED RUBBER PRODUCTS Joseph C. Elgin, Princeton, N. J., and Edward F. Sverdrup, Buffalo, N. Y., assignors to U. S. Rubber Reclaiming Co. Inc., Buffalo, N. Y.

ApplicationFebruary 3, 1951, Serial No. 209,287

27 Claims. (01. 260-23) This invention relates to the reclaiming of rubber and to reclaimed rubber and to products formed from or containing the same.

This application is a continuation-impart of our copending application Serial No. 193,688, filed November 2, 1950, of our copending application Serial No. 44,017, filed August 13, 1948, as a continuation in part of our copending application Serial No. 39,476, filed July 19, 1948, and of our copending application Serial No. 695,630 (now abandoned), filed September 9, 1946, and of our copending application Serial No. 727,275, filed February 7, 1947, which is a continuation-in-part of our application Serial No. 524,064, filed February 26, 1944, and issued as Patent No. 2,415,449, dated February 11, 1947. Application Serial No. 727,276 was abandoned subsequent to the filing of application Serial No. 39,476; application Serial No. 39,476 was abandoned subsequent to the filling of application Serial No. 44,017; and application Serial No. 44,017 was abandoned subsequent to the filing of the present application.

An object of the present invention is the provision of a process for reclaiming vulcanized natural and artificial rubbers whereby greatly im-. proved economy and an improved product may be obtained. A further object is the provision of a process whereby reclaimed rubber of uniform quality may be effectively and expeditiously produced in quantity. Another object is the provision of an improved procedure for reclaiming mixtures of vulcanized materials. Another object is the provision of greatly improved reclaimed rubbers which approach the unvulcanized polymer in workability and utility, which has itself unique fields of utility, and which, alone or in combination with other ingredients, can be readily and effectively vulcanized or otherwise converted to a product which will have a long and effective life in any of a wide variety of useful applications.

In accordance with the present invention there is provided a continuous flexible process wherein all parts of the rubber progressively are subjected to a treatment adapted to devulcanize, i. e., to restore aplasticity similar to that of unvulcanized rubber, and the treatment in each part is terminated before the rubber can be undesirably affected. Thus, there is produced a reclaim of uniform quality and at a continuous rate. This process when used in the controlled-short-period process and the special oXido-reclaiming agents described and claimed in our Patents 2,415,449 and 2,593,279 among others permit a greater efficiency and improvement on said inventions by bringing each part of the rubber to the desired point on its plasticization curve and then arresting the action.

In accordance with the'invention there are provided reclaims which have a high plasticity (a low Mooney viscosity) and, when vulcanized, a high tensile strength, a high percent elongation, and high abrasion resistance qualities (a low abrasion loss), and which have in certain instances a low thermal softening factor, a high capacity for assimilating such materials as clay and carbon black, 2. low power requirement in assimilating a load, a high degree of softness and smoothness, good processing and compounding characteristics, good extruding and tubing characteristics, and potentialities, when suitably compounded, of being vulcanized to a product having a number or all of the following qualities: 2, low torsional hysteresis loss, a long effective life, a high resilience, and/or a low torsional hysteresis loss, and long life; and other products having highly improved qualities.

Distinct characteristics of our product are that it possesses a consistently high quality factor as I expressed by the ratio wherein T stands for tensile strength of the product when cured, E stands for percent elongation of the product when cured, L stands for abrasion loss of the product when cured, and V stands for Mooney viscosity, consistently high ratios, and consistently low abrasion-viscosity factors represented by L V, all when compared with the products of other processes produced from comparable vulcanized scraps with comparable quantities of the same type of added ingredients under comparable temperature conditions.

Reclaimed rubbers such as contemplated by the invention are identifiable by the presence of certain or all of the above and other qualities including good Working characteristics, a relatively low gel content, a low swelling index, a relatively high resistance to water dispersion, a high cured chloroform extract value, a high softness and smoothness which do not interfere with the processing characteristics of the reclaim or the desirable properties of the vulcanized product, and, when vulcanized, by a low T-50 value. When suitably compounded and vulcanized, they yield products which are outstanding in desired ones ofthe followinglqualities in high degree; resistance to abrasion, low torsional hysteresis loss, and im roved aging characteristics; their tensile, elongation, hot tensile, and flex resistance characteristics are high; and their hardness and modulus characteristics are good. They serve for use in tires and for other purposes as a highly satisfactory equivaleni'; of raw rubber in. admixture with synthetics and otherwise. They provide bases for products having outstanding utility in many industries, and they have qualities which: to:

enable their use, per se, for a wide. range of. purposes.

It will be appreciated that, as is the case with all rubbersnatural. synthetic, and reela-i-m-the properties of the vulcanized product will vary in accordance with the compounding and treatment. Different qualities are, required 01". tube, tire-tread, side wall, carcass, mechanical oods, and other products; and the compounder will seek and obtain high qualities in those factors which are particularly important tor the. use: to which the product is to be putt. For example; high abrasion resistance and low hysteresis loss areboth important tire-tread products; whereas, .in. carcass products, low' hysteresis: losswould be of even more importance, but abrasion: resistance would be of substantially no.- importance. The compounder who is seeking, low hysteresis loss will design his.- compound to favor factor rather than high abrasion resistance, whereas the compounder who is seeking high. abrasion resistance will design: his compound to favor the latter; By means of the present invention, however, the compounder who is seeking a low hysteresis loss factor is able-to secure a vulcanized product with an exceptionally lowhys-teresis loss, and the compounder who is; seeking a high abrasion'resistance factor will be. able to obtain an exceptionally. high. abrasion resistance. Improved aging and other qualitiescan also be obtained. The reclaim of the present invention has potentialities for use in exceptionally high quality vulcanized products embodying variouscombinations of desirable factors the most desired ones of which are present in an outstanding degree.

The reclaim of the invention may b identified, in certain instances, not only by characteristics such as just discussed, but also by other factors such, for instance, as its low Water diSpersl-on characteristics when milled. with ingredients which convert standard. reclaims into products which will disperse readily in the presence of water; and also by its low- T-Sdvalues. T-5Il values, as is well known in the art, are obtained by freezing an elongated sample of vulcanized rubber stretched to about 75% of its ultimate elongation. When it. is thoroughly frozen, the clamps are released and the T-50- values are basedv on the temperature at which there has been sufficient thawing to return the sample to 50 of. its original stretch. The test is also known: as A. S. T. #13599-40'1, a description. of which may be found on page '76 of A. S. T. M. Standards on Rubber Products for March 1946, and a discussion of which may be found-in Critical Analysis of T-50 Test in the India Rubber World for November 1939. Surprisingly, the reclaim of the present invention, when vulcanized in a usual manner, gives, at or near optimum cure, T-SQ valu s considerably lower than standard reclaims, indicating that the product, instead of being merely a further development of known products, is a uniquely different material.

While special reclaims have in the past been obtained which were particularly high'in certain particular ones of. the above qualities, our reclaims tend to run consistently good in the foregoing and other qualities when compared with reclaims produced under comparable conditions by other processes.

The product of the present invention is believed to have a higher average molecular weight, narrower molecular weight; distribution, and a less highly-branched, cyclicized and cross-linked structure than the standard reclaims hitherto available.

We have found that these results are best obtained whenthe vulcanized rubber thoroughly mixed with the reclaiming agent (with or with out. other ingrediemss: affecting the properties of the product): is. passed continuously and progress-ively a closed apparatus in which it is heated, mechanically worked with a shearing action controlled so as to avoid actual shear-i. e., laminar fracture with consequent slippage of contiguous parts of the'rubber mass relative to each other along their surtaceofcontact-is protected from; the atmosphere while-hot, and aiter. a relatively very short period of treatment, is cooled. before, or as, itis discharged into theatmosphere.

It is: important to-give all: parts of the Vulcanized scrap full heating and working, and this can be. advantageously accomplished, according to the present invention, by repeatedly passing. the material thru clearances so small-as to-assumemechanical. working of. every particle: and; intimate contact thereof. with a. hot. wall over which. it is moved After each. such passage, the material. is extruded into a larger space where. the material is mixed. and. allowed time for action of'heat and.

a reclaiming agent. before being forced thru the next narrow clearance. The adjustment of the clearances and the number of. points of close clearance controls to a large extent the quality of the reclaim and the production rate; the more points of close clearance, the. less chance there will be that, any particle can passthrough the device without, full treatment substantially equal to every' other particle- Refining oflthe. stock. can be done in this same process, or, if desiredthe stock maybe given a further refiningas in stand.- ard reclaiming practice.

The invention accordingly comprises-an article of manufacture possessing the features and properties which will be exemplified in the article hereinafter described and the scope of the appli cation of" which will" be indicated in the claims.

For a fuller understanding'of the nature and objects of the invention, reference should. be had to the following detailed description taken in connection with the accompanying drawings, in which? Figure 1 is a sectional'view of one type of product embodying the invention;

Figure 2 is a longitudinal sectional View of one form of" apparatus wherein the product may be produced; and

Figure 3 is a longitudinal sectional view of anotherform of apparatus well adapted for manuiacture of: the product.

The reclaimed rubber of the invention, as shown, for instance, in Fig. I, is of greatly improved quality and has characteristics which are unique in the rubber reclaiming art.

'One manner of. production of such material of uniform qualityand at a continuous ratev is illustrated in Fig. 2 wherein the material to be reclaimed is supplied, in admixture with reclaiming agents and other ingredients, to a hopper'i having a feed opening 5 The -material, still substantially at room. temperature drops fromthe hopper 5 into a tubular chamber '6 in which is a screw type rotor I. This screw is connected to suitable driving means through the drive gear 8 and speed reducer 8'.

In certain longitudinal portions of the chamber 6, there are provided, on the rotor, flights 9a and 91) having sloping, rounded contours, designed to provide for working of the material, thus permitting a portion of the material to work over the flights 9a and 9b. In other longitudinal portions of the rotor, its flights III are designed as a typical forcing screw so as to engage the ma terial and feed it continuously along the cham her 6. The clearance at the tops of flights 9a and 9b may be a; of an inch. The depths and differences in contours in the several portions of the rotor are designed to produce mechanical working of the material while maintainingit in intimate relation with the wall of chamber 6, the temperature of which is controlled by fluid circulating in jacket portions II, I2 and I3.

As exemplified in Fig. 2, whereinthe parts are drawn substantially to scale, the three-inch diameter screw thread is formed to provide two "plasticatin'g sections 9a and 9b flanked by three forcing sections II! as indicated. In these sections heat is rapidly developed by mechanical working of the material and friction against the movingparts, which provides (in connection with external heating or cooling if desired), the appropriate reclaiming temperature, e. g. around 400 F., or other temperature within the reclaiming range.

The temperature of the chamber 6 is controlled in the present instance by a jacket in which a suitable heat exchange fluid, e. g., oil, Dowtherm (eutectic oi diphenyl and phenyl ether), or even steam, is circulated. As shown, three chambers II, I2 and I3 surrounding the conduit make up the jacket for the chamber 6. A heater is provided in the thermostatic storage tank I5 for initial heating-up and for boosting the temperature of the heat-exchange fluid, if internal heating of the material should be insufficient. In operation, however, it is best to heat by mechanical working so that the jacket actually carries oil heat and serves mainly as a temperature control means. The fluid runs through pipe I6 to chamber I I, through pipe I! to chamber I2, through pipe I9 to an auxiliary or step-up heater 2n, and thence through pipe 2| to chamber I3, return ing to the thermostatic storage tank I5 through pipe 22. A pump (not shown) may be used. At the discharge end of the screwpart of rotor I and chamber 6, is an extrusion section oomposed of a conical extension 25 on the rotor I and an extension 25 of the chamber '6. The clearance between these parts is such that only well plasticized rubber flows through it, and such rubber is cooled by intimate, contact, in thin section, with the wall. 26. By virtue of the conical form, this section provides smooth tubular flow, and prevents laminar flow; but it is advantageous to 'increase the clearance progressively as the diameter decreases so that the area of the annular opening remains constant or even increases toward the small end of the cone. The area of this orifice, and, to a considerable extent also, its temperature, control therate of flow of the material being treated.

From the zone 21 the material gathers in a chamber 31, whenceit passes into the annular chamber 32, in which it is then subjected to fur-'- ther compacting by extrusion through the an nular orifice between the cone 33 and the cylinder. This is adjustable by turning nut 36 on the threaded pin 35. This also produces back-pressure which affects the rate of flow, and assures the exclusion of air.

In the zones 21, 3| and 32 the temperature is reduced, by external cooling, from one within thereclaiming range (of over 325 F., e. g., 325- 425 F.) to one not over 325 F., and preferably lower. Dissipation of heat generated by mechanical action during extrusion through zone 21 and some cooling of the stock below its temperature in the active treating zone is thus carried out in zone 21.

.The cone 25,'the tube 34 and the conduit 3| are, respectively, cooled by jackets 39, 40 and 4! through which a cooling liquid, e. g., water at controlled temperatures, e. g. at about l75-l95 F., is circulated from pipe 4| and by pipes 42 and 43. A discharge pipe 41 runs from jacket II to a recycle cooler and pump or to discharge.

The apparatus is drawn substantially to scale in Figure 3 for a 3 outer diameter screw. The space 27 between the cone 25 and the tube 26 may be about 0.030, but is adjustable by the bolt 313 engaging nut 30 secured to the bed of the machine. The orifice at the outlet of chamber 32 may be 2%" in external diameter and 2 5%" in internal diameter.

We have found that the best results are obtained when the vulcanized rubber, thoroughly mixed with the reclaiming agent (with or without other ingredients affecting the properties of the product), is passed continuously and progressively through a closed apparatus in which it is heated, mechanically worked, protected from the atmosphere while hot, and, after a relatively very short period of treatment, is cooled before, or as, it is discharged into the atmosphere.

Best results are obtained by the use of screw means in a jacketed tubular vessel, whereby the material is treated in an annular passage between the screw and the vessel by repeated extrusion over the thread of the screw. The material in the tubular vessel or other heating chamber is advantageously maintained during treatment at a temperature known to be efiective for reclaiming the particular materials being treated. Advantageously the material is treated in intimate contact with a channel wall held within a temperature range from approximately 390 F. to approximately 590 F. during the active treatment, and thus the temperature of the stock during treatment is kept under close control. Each part of the stock, in turn, remains under such temperature conditions for substantially the same time, which for best results should be not substantially less than one minute nor substantially more than twenty minutes. Reducticn of the amount of reclaiming agent below an optimum amount (or its omission) requires higher temperatures; whereas with the preferred devulcanizing agents, softeners, eta, lower temperatures and higher working speeds can be used. Increasing the temperature above 400 F. adversely aiiects the tensile strength, but it does make a softer stock.

Heating is direct and internal, clue to the internal mechanical working- The energy input rate for the types of material given below is advantageously of the order of 1.0 to ill horsepower hours per pound of rubber. It is an important advantage of this invention that during continuous production this power input remains substantially constant. ,In its more 1, specific aspects. the inventin. contemplatesan energy input relative; to the flow rate; of. about .15 to .83 horsepower hour. per pound.

The stock after it leaves the treating: zone should be cooled substantially below the; treati'ng temperature, in most instances below about 350: E, and advantageously below 3.00 F. As soon as possible after the rubber is discharged into. the open atmosphere, it isv advantageously cooled 'to approximately room temperature.

Rates of feeding and. forcing of the. material into and. through the feeding zone; within the: limits stated, depend to considerable. extent upon the nature of the material being treated and of the: added ingredients, the temperature at which the treating zone is maintained, the severity of the mechanical working to which the material is subjected, and'the: kind of product which is desired. For ordinary rubber reclaimingand using the preferred ingredients as specified herein the rate of flow is. adjusted to give a time in the treating zone of two to three minutes.

Usual reclaiming agents may be used. The process is most advantageous, however, with the oxido-plasticization agents described in the prior applications mentioned above, or with other agents which tend to be effective in the splitting of rubber molecules and/or in controlling crosslinking. In particular, the invention in its more specific aspects contemplates the provision of products in the production of which lauryl triercaptan or other aliphatic mercaptans having not less than nor more than 16 carbon atoms (for example, decyl, undecyl, lauryl, tetradecyl, or hexadecyl, mixtures thereof, or mixtures includin one or more thereof). The use of branchchain compounds (especially the tertiary compounds), gives especially desirable products. Excellent products also are those produced by the use of disulfides, thiop-hene compounds, etc.

ther materials may be used, such, for example, as mineral oils, pine tars, coal tars, resins, etc. Naftolen R400, a commercial resinous product recovered from acid sludge of petroleum refining, Staybelite Resin, a hydrogenated rosin product in common use under that name, B Wood Rosin, Phillips Reclaiming Resin No. 1, a petroleum resin commercially offered tothe reclaiming industry, stearic acid, oleic acid, 2-ethyl buty-ric acid, styrene monomer, may be used with good results.

The material to be rendered plastic-for instance vulcanized natural rubber, Buna S (GR-S), neoprene, other diolefin polymer materials, butyl rubber, or mixtures thereof with each other or other materials, but advantageously free from textile fabric cord, etc.- should be premixed in coinminuted form with desired oxido-plasticization agents and/or other d'evulcanizing agents, softeners, etc, at a temperature sumciently low to avoid deterioration, preferably not over 250 F., and advantageously in presence of air. The mixture should be supplied to the reclaiming apparatus in finely divided form. The vulcanized rubber scrap should be cleaned and ground in the usual way, advantageously to a fineness of i2, 24, or, better, 36' mesh, and be free from metal or other foreign ingredients which might injure or interfere with the reclaiming apparatus. This crumb rubber, mixed with reclaimingagents, softeners, etc, is supplied in sufficient quantity to keep the working space of the reclaiming apparatus filled and ta'maintain a continuousfiow'through it. When oxido-plasticizing. agents according-to the said prior applications are-used in the present process, they are advantageously premixed with the stock in thepresence of oxygen, at temperature below about. 250 F. In general, however, it. is feasible also to supply all materials continuously in. proper proportion and to. rely on the mechani-.

cal workingof the plasticator apparatus for mixing. 1

By mixing with an oxido-plasticization agent in the, presence of air, sufficient oxygen for activating the; agent; so as to. bring about the desired plasticizin'g; reactions including chain-scission is incorporated, and when'the material enters; the reaction chamber-it is compacted by the. worm, and the. reactions occur in, the; substantial absence of:' air-1 Thus the. oxidation reactions. are controlled, and the material protected against excessive oxidative degradation.

Once the desired reactions have taken place, the product should; becooled quickly to bring about. the transformation of the material from its reactive state to a stable. condition. When the: treatment is complete, the material'is cooled by extrusion through a cooled orifice; or the hot material may be extruded into a cool inert gas (e'. g. CO2): or a cooling liquid, such for example as water, which may be flowed or sprayed or merely maintained as a. cooling bath. The treated material may also be fed down into: a standard cool mill; or cooled by other suitable treatment. Storage temperatures should be not appreciably above room temperature.

In the provision of the products contemplated; by thepresent invention in its broader aspects, noparticular form of apparatus or treatment is essential. Furthermore, a machine may be. varied considerably so long as the extrusion orihas is. sufficiently small with respect to the worm capacity" so that't-he material will be compacted within the chamber'by the worm so as to sub stantially exclude air, and so long as working aswell asaforcing. of the material is achieved.

Certain of the products exemplified hereafter were made on a machine such as: illustrated in Fig. 3:. The worm diameter is six inches (instead of three inches), with the other dimensions drawn substantially to scale in Fig. 3. The parts v are designated by reference numerals such as those used in Fig. 2, but preceded by 10 in the case of single digit'numbers, and by 1 in the case of double digit numbers. Thus, for instance, the machine includes a hopper I05, a tubular workingand forcing chamber I06, and a worm I01. Besides. the temperature-control chambers III, H2, H3 there are inserted, between the chamber I I2 and the chamber II3, twochambers 2a and H212, respectively. Piping II'I connects the chamber IIZ with the chamber II2a, piping I-Ila connects the chamber I I2a with the cham ber H212, and piping I I'll) connects the chamber H 211 with the chamber I13. A-cone I25 and chamber-extension I26 are provided, and between. the-outer wall of the cone and the inner wall of the chamber IZGais an orifice I21; and there is: a furtherorifice i32 between the outer surface of a. cone I33 and the inner surface of a tube I34. The chamber I3I' is fore-shortened,-

and the temperature-control chamber I40 is formed: in the tube I34. Internal cooling means in the form of an inlet tube I50, a cooling chamber :51, a return I52, and an outlet I53 are provided.

There is given below data onthe screws'oi the machines of Figs. 2 and 3:

Fig. 2 Fig. 3

Length 7% Valley depth i tapering is" tapering to 362. to z. 1st plasticating section:

Length 6 13%. Valley depth. z. 2nd forcing section Len 10. Valley depth %2. 2nd plasticating section:

Len h 13%. Valley depth. %2. 3rd forcing section Length 11%. Valley depth %2.

Using the machine'of Fig. 3, flow rates of between 280 and 300 pounds per hour have been obtained with an oil temperature through the piping i l6i22 of 280 F. at an oil flow of 9 gallons per minute. Temperatures below 280 F.

tend to lower the rate of extrusion, and temperatures as high as 330 F. have tended to result in unsteady operating conditions. An oil temperature of 320 F. is desirable if the oil flow is raised above 11 gallons a minute. The water fiow rate in the piping l4! '--l41 is desirably between one and one and one-half gallons per minute at a temperature about 208 F. for a production rate of 280-300 pounds per hour. Flow rates as highas 400-500 pound range in this machine are eifective in yielding the product of the invention.

By way of showing certain advantages of the invention, certain comparative data are given hereafter. For this purpose a standard reclaim is here identified for purposes of later comparison.

STANDARD A standard commercial reclaim made by treating natural rubber peels in pans for five hours in open steam at 363 F. following a gradual rise in heat during an initial hour and one-half, refining twice, straining through 70 plate, and finishing at a maximum gauge of 0.008 inch was used.

This, mixed with 50% of fresh GR-S compound and vulcanized for the number of minutes and at the temperatures indicated under Cure below, gave the results indicated under the word The above mix was processed in the plasticator of Fig. 2 at 40.2 pounds per hour at a temperature of 350 F., worm speed 104 R. P. M. The process time (for each part of the product) was about 4.73 minutes. a

10 Example 1 The product of Process 1.

DIRECT ABRASION TESTS (REOLAIMERS' ASSOCIATION FORMULA) Standard" Example 1 Loss in Hardness LOSS in Hardness cc./HPH cc./HPH

' 4m? s07 57 645 50 so 4o# s31 as 675 52 5/0-E paper, (Cutrite Production paper, lot U538T) was used.

The Reclaimers Association Formula (some times abbreviated as RAF) is as follows: Reclaim (50% hydrocarbon) 200.00 Zinc oxide 5.00 Captax (mercaptobenzo thiazole) 0.50

D. P. G. (di-phenyl guanidine) 0.20 Stearic acid 2.00 Sulfur 3.00 The cures as indicated are for 25 minutes at 40 1 pounds of steam (287 F.) and at minutes at 40 pounds of steam.

The abrasion tests set forth herein were performed on a machine such as disclosed on pages 674-677 of volume 19 of Industrial and Engineering Chemistry.

PROCESS 2 Parts by Formulation weight 35 No. 1 Natural rubber peels (tire treads peeled from the carcass) ground to size adapted to pass a ZeL-mesh screen 95.00 Tertiary dodecyl mercaptan. 50 Petroleum solvent (Solvesso No. 3*) l. 50 Engine oil (Topsall No. 62) 1. 50 Lecithin (clearate) .50 Water 1.50

Pr0cess.48 pounds per hour in the machine of Fig. 2, which corresponds to 3.87 minutes at 365 F. The Worm speed was 48 R. P. M. The stock was refined once at .0035 inch maximum spacing between refining rolls.

A high aromatic petroleum naphtha of boiling range 34 54l0 F. with a specific gravity of 0.883, an aniline po nt of 22.7, a flash point of 130 F., an initial boiling o1 n t of 347 F., a 50% boiling pointpf 373 F. and a final Olhllg point of 412 F. and containing aromatics.

7 Example 2 The product of Process 2. Chemical analysis:

Abrasion loss Cured with 50% RA 5/0-E paper) 11 A product of Process 2 gave a Williams plasticity of 4.84, a Moon y viscosity (ML/'l3Q/L5 -1) of 71,=a Mooney viscosity (ML/ 212/6/1) of 58, (ML/180/6/1) of 70 (both Mooneys taken ten days after reclaiming), a thermal softening fac- 5 refining r 11 tor (change in the last two. Mooney viscosities Example 3 with temperature of .375. -ML signifies that r r V the larger of the two standard Mooney rotors was The product of Process 3. used. 180 or 212 indicates the temperature s'oft Smooth reclaim having, a ,Wib in degrees Fahrenheit, the first figure thereafter v hams blasficitynl'nnber of 431 at C). indicates the warming-up time, and the final V figure the time of the test). When cured (RAF Chemical analysis: 50%, i. e. where the. reclaim cont s 5 e- Acetone extract 21.45 carbon) it gave an abrasion loss as follows: (in u i d extmc 4536. this test Minnesota Mining paper 8/ 2 0, l Ash V 7 4, 3 UT4 aluminum oxide grit was used in this and the Total sulfur 1175, following examples. Abrasion figures obtained Carbon G with 5/0-E paper may be converted substanbe '4 tially into figures for 8-[0-280 paper by dividing hydrocarbon 3695' by 1'35.) 7 y--==f-=.-a= flfifinwf zv Tepsfle Eloggafigg Abragssion v ggrqllgsg Cured in Reclaimers Association For 25' at 40# i 5,18 47 i Abrasion 30' at40# 1, 248 320 497 49 2e Tensile V Y Hardness fig The quality factor is calculated as follows-: at 287 s04 423 40 at 287=F-. 012 331 4 1 012-v 1,248 320 3 a 287 0 .4 3 3 9 A torsional hysteresis figure 01 0.086 was ob- After a thirty-minute cure (RAF 50%) a tortained. sional hysteresis figure of 0.110 was obtained.

A product of Process 2, having a Mooney viscos- A product of- Proc 3, having a Mooney visity (ML '180/L5-1) at the time of load testing, of cgsity 9,1; t ti of m te ti ML/1 0/ 1 5/ 71, assimilated. 500 ams, Q 115 38019 31 D l 1/1-7)-i-. e., measured seventeen days after regrams of reclaim, on a 12" x 6" mill of 1:1.3 roll i i of 71, i il t 700 grams of s ratio, and required a maximum 4- 9 horse-e clay per 500 grams of reclaim, on a 12" x 6"" mill, p w r W il mixing in t last 0 gr s. of t and required a maximum of 5.37 horsepower while amount, and a maximum or 4,251 horsepower when mixinginthe last 100 grams of this amount, and the load was all mixed in. (4% of stearic acid a xi um of 5.04 horsepower when the load was added on the clay.) was all mixed in (4% of stearic acid was added When this compound was, vulcanized: (1% of on the clay). When his, eeme (Containing Zenite A, of stearic acid; 3 of Z nc oxide, the clay) was Vulcanized (1% of Zenite A, 1% :of and 3% of sulphur, h d e n added on an ass eari acid, 7% 0i. zinc oxide a d 3%. f; lfur sumed RHC-rubber hydrocarbon. content of hag be n added on an assumed rubber hyd Q- for 10 minutes at 307 F., the durometer reading carbon content of; 50%) for 10 minutes at 3075* F'., as 83, thetensile s r n th wa 92.3 pounds, and the durometer readin (hardness) was 35, the the elon ati n was 1 ensi tre th waS'53.5 p- (pound per square 50 nch ,and t e. el n t on was 80% PRGCESS 3 This product had a thermal softening factor .88 erir d rom Mc neys MAS N/114. i; l .1 4 1 ML/ 2 12/6/ 5 .v of 5-55 Formulation 32%? Whe arts by W i ht of; the, standard.

ee aimindieatedgaPQVeis seQ ta 00 n rts qf; N04 GR S peelsground t 24 11 11 95.00 the type of rubber Indicated t 1. 3415 f, th 'eRt%&I1-\$I od(ige((g]11fililieI)apt8H columns below in a compound suitable for tire Petroleum solvent f loiidrifnaphtha l. 50 sldewan, and the reel-almp s 2 nd 3 L cithin (clearate) are used with the type of rubber indicated at the heads of the columns below and in an otherwise 1 respectively similar formulation and tested com- A petroleum resin containing about non-volatile paratively, the following results are obtained: solids, having an initial boiling point oil- 38 03 F. and boil- 7 ing point of 160 F. after 20% distillation, and having an iodine number of 190, an API gravity of 15-18, a specific i ?ta% I3 'F $$332115;fit iiifi's ag e e r Ema iorn igrz gr. Wt. 100 rev.-sec.'35 -'-40)I O rub ge i W1 ru a 5 ure alial iyslg rd rubber makersclay having approximately the. following Tensile g ga t i,n Tensile SE31; .Tensue 51%;!

Loss on ignition "7..-, 14.00 Silica. 7 .50 7o 20' at al 2,680 530 2, 900 520 2,680 565 Iron and aluminum oxides 43-00 305 at 45% 2, 480. 490 2,800 52 0 2, 840 570 Calcium oxide 1. 50 45 at 45# 2. 2, 370 40s 2, 700 520 2,700 540 Magnesium-"r None 90' at 45#-.,- 2, 050 470 2, 020 540' 2,380 5 rfilteisssi esngeification is: less than0.5% retained ona200 mesh e T 300,, tests below ep ese m d u Macrame-43:5 poundstper hour in'the'macliine of Fig. 2, which corresponds 1104,21. at 3&6. F: The worm speed Was 60 R. P. M. The stock Was refined once at .0035 maximum spacing between characteristics, i. e., tensile at the point where the elongation is 300%.

Cure T300 T-300 T-300 HOT TENS ILE (212? E.)

I Elon- Elon- Elon- Oure Tensile gatlon Tensile Eamon Tensile gation 20 at 45# 1, 380 550 2, 120 650 1,960 690 30 at 45# l, 340 520 1, 740 580 1, 875 650 350 520' ,850 580 1, 710 640 1, 300 575 1, 700 565 1, 460 655 AGED 95 HOURS IN OXYGEN BOMB Standard" Example 2" 1 with natural with natural ifi fi ggj rubber rubber Cure Elon- Elon- Elon- Tenslle gauon Tensile gation Tensile gation 20' at 45# .1 1, 870 390 2, 150 430 1, 960 475 30 at 45# 1, 720 370 1, 650 380 1, 875 440 45 at 45#. 1, 580 350 1, 760 360 1,710 410 90 at 45# 1, 480 335 1, 760 385 1, 465 400 TORSIONAL HYSTERESIS 0. 066 l o. 061 0. 067 065 057 06B O68 057 067 076 065 075 PROCESS 4 Parts by Formulation weight Peeled #1 tire recaps (24 mesh) 95. Tertiary dodecyi mercaptan. 50 Naphtha (Houdry) 1. 50 Petroleum resin (Phillips PRR #1) 8.00 Lecithin (clearate) 50 Water 1. 50

Process-45 lbs. per hour in the machine of Fig. 2, which corresponds to 4.13 min. at 364 F. The worm speed was 60 R. P. M. The stock was refined once at 0.0035" maximum spacing between refining rolls.

Example 4 The product of Process 4. The qualities of this reclaim asv evidenced in a compounding with natural rubber similar to that of the tests immediately above are listed below in comparison with Example 3compounded similarly.

HOT TENSILE (212 F.)

Tensile Elongation Tensile Elongation 20 at 451? 2,030 725 2, 030 670 at 1, 650 620 l, 440 565 45 at 45# 1, 900 640 1, 760 620 90 at 45?! 1, 600 610 1, 320 525 Cure Example 4 Example 3 20 at 45# 10.8 8. 8 30' at 451% 20. 2 16. 8 45 at 451% 23. 3 -20. 7 at 451* 25. 5 22. 8

PROCESS 5 l Parts by Formulation weight 24 mesh natural peels 95.00 Tertiary dodecyl mercaptan" 50 Engine 011 1. 50 No. 132 solvent 1. 50

7 Prooess.--In the machine of Fig. 3 a rate of 380# per 110111 at 40 R. P. M. (2.3 at 395 F.)

Example 5 The product of Process 5. When parts by weight of the-product are mixed with the following compounding ingredients:

and cured for the number of minutes indicated in the first column below at the temperature of saturated steam pressure indicated in the second column, there are obtained the following results:

Cure

steam '1 E H 150, 0. Minutes pressure,

pounds Here and hereafter T=tensile strength, E=elongation and H=hardness.

After-a thirty-minute cure (RAF 50%) a torsional hysteresisfigure of 0.085 was obtained.

In comparison with the above results for Example 5 there are given similar figures for the standard pan process reclaim, the stock being identical, and the reclaim being similarly compounded.

'r E H 1 50, o o

20'/40# 1, 005 290 49 33.3 1, 004 270 51 33. 3 1, 094 267 53 -33. 5 1, us 251 55 34. o

, A product of Process 5, having a Williams plasticity of 5.38, and a {Mooney viscosity (ML[ 1.5- -1- -1) at the time of load testing, of

gamma 64', assimilated BOO-grams of Emprex clay per 500 ratio, and required a maximum of 4.51 horsepb'we'r'while mixing in the last 100' grams of this amount, :and a maximum of 4.51 horsepower when the load was all mixed in (4% of stearic acid was added on theclay) A thermal softening factor -o1 .375 was obtained for this product from Mooneys (ML/'180/6/1/17) or 68, and (ML/21'2/671717) of 54.

When'this product was vulcanized (1% of Zenite A, 1% of stearic acid,3% ofzinc oxide. and 3% of sulfur, had beenadded on an assumed RHC of 50%) for 10 minutes at 307 F., the durometer reading was '82, the'tensile strength was 868 pounds and'the elongation was 100%.

Below are shownthe results "of comparative test "on red inner tube reclaim .random scraps:

'PRO'CESS '6 I JParts by Formulation weight 12 mesh red inner tube scrap... 100.00 Tertiary dodecyl mercaptanfln $50 No. 132 solvent 1. 50 Water 1. 50

Process-2.25 min. at 390 'F.; equivalent. Produced at a rate of mopoundstperhour *the machine of Fig. 3. The worm speed was 140 R. P. M. Finish 0.0035" max.

Example '6 stearic acid substitute manufactured by Wilf zge y p sing carbon) 35. mington Chemical Company), and 5.0 parts ofgggg g ethanolamine, and treated in aipan for6 /2 hours. g g ge x 1.100 Durin the first hour and 0neha1f t r 33125319.: f? .?3?f?:::::: S232 ture rose gradually to 363 F. and was main- 5 p l v1300 tained at this figure for the remaining five hours. It was refined twice, 0.004 and 0.0025".maximumf gauge finish.

The cures were all made in the following 'for- Standard Example 5" mula: 55 'Gure I I "'Ien T4500 Elon-' Hard- "I-cn- T4300 Elon- Hard- Redaim 0% rubber hydrocarbon.) .1 50 5116 gallon 11658: $119 figatlolli 11955 Zinc-oxide.... CH HT. or- 3.00 j I ggg ggggf gg gz 1 3g 45at 280 F. 2,781 1,491 477 63 2, 744 1,2088; .520; =59 sulfuruimn :LSO eomzsmr. 2,733 1,514 450 65 2,736 1,386 487 60 Steam ML" 120 75at280F 2,675 1,626 433 64 2,71? 1,453 470 60 106-42 "ToRsroNun-HYsTEREsIs ii'rzss F.

our? Standard" Example M 4'5'at 280 F. 0.163 0.1 53 'r-so, 0. 'r-so, 0. 60 Et1280(F .167 .:15s n e5 75at280F -171 .166

57401115 -35. 1 aas -44.

36.0 #44,? 11 401115 --4o.0 145.2 Formulation C is .the same as .formulation p B but with 60.00 parts of GR-Ssubstituted for 70 the 60.00.,parts .of .smokedsheets and with .thesul- A product of Process 6, having Mooney viscosities taken eight days after reclaiming (ML/=180/L5- 1 of 56, (ML/18073 of 51, (ML/-1 80/6-1) of 46, (ML/ 212 /1i5-1 ofl'l'and (ML-A2 li2l-3-l (if 42, and MB/Zl-ZfG-D of 42.

i6 This product had a thermal softening .factor of 0.13 between (ML/180/6-1) zan'd '(ML/.-2'l2/6-L)..

C OMPARATIVE DATA Test Formula 'A":

Reclaim 00 19-33 .carb on 00 Pineitar .00 Zincnxide. .50 Sulfur .50 .Mercaptob z fhia'mlp Di-phenyl guanidinenufi l. 10 Stearic acid 1. 00

Standard Examplefi ure e .t e

. l ine cent S Pep cent S, pep

cent f cent 20.at 40# .i -'81. 3 0.353 23622 g -.34. 3 0. 413 2. 560 c086 25838 -.34.=5 .155 2.818 .1068 2. 857. -34. 0 093 2. 880

Specific gravity.- l.169 1.161

ABZRASION Standard Example? Cure V v I i Hardness Hardness 20 at 40# 892 52. 892 4.0 40 at 40# 820 56: 760 48 at 40% 834 58; 690 48 Further tests were made with a 'treajdtype compound usingznaturalrubberz fur reduced 1:02.25 parts.

STANDARD #5015 I The following data is for #1 Peels Recaps 'for another Stand-91rd Dan process reclaim (designated as #5015): 1

GR-S COMPOUND-FORMULATION "(1 30' at 280 F 854 50a 54 502 975 510 55 552 45'at2s0 F- 1,514 557 58 755 1, 586 527 55 75s Formulation Partsbv 50' at 250 F. 1, 547 510 50 957 1, 855 453 59 1, s we t 75' at 250]? 1,959 480 51 1,055 1,995 '477 50 1,095 90' at 250 F- 1, 950 470 50 1,154 1, 951 475 59 1,117 No. 1 recap peels)? 100.00 No. 13 2 s0lent i- NATURAL COMPOUND-FORMULATION B 8: :40 [Torsional hysteresis at 285 F.] g g e ,g-% 16 woe mm 180,00 45'81; 230 F. 0.217 0.194 water A v 50' at 280 11 .214 .101 75at280F. .220 .107 Process.-.-5 hours at 388 F. 4 Mill as: g j GR-S COMPOUND-FORMULATION "0" Product of above 97.0 15 [Torsional hysteresis at 285 E1 Clay 3- 1 Refine -00 and -0025" Cure StandardNo. 5015 Example 7 Finish .007. j

5 55: 15 "-15 5. .7 With this may be compared. 20 7521290 F .178 .150

P OCESS 7 R CURED CHLOROFORM EXTRACT No. 1 recap peels 24 mesh 95.00 Tertiary dodecyl mercaptan i 1.00 gfggg? "11115111 1157" No. 132 Solvent l 1.50 25 PER No. 1 9- 108% 248% Process.3 at 410 F. 300 #/hr. 40 R. P. M. in the machine of Fig. 3. GEL CONTENT Refine.-.0O" maximum. 6

, 7, Example 7 M 3323 55 Example? The product of Process 7. These reclaims were tested in the same way as the natural rubber peels 5% 9% given above. In tests using Test Formula A above, the following results were obtained: SWELLING INDEX 5 Example7" Standard #5015" Example 7 Cure 515 734 Ten Elon- Hard- Ten- Elon- Hardsile gation ness sile gation ness 20740;; 1,075 550 51 821 577 42 40'/40# 1,170 333 56 924 330 46 Cure "Standard No. 5015 Example 7 507401 1,197 353 55 920 320,. .45

0. C. AGED 24 HOURS AT 100 0. 20' 21 40#.. 27.5 -29.9 '40'11140# -25.5 -2s,0 50' at 4011.-.. -24. 1 -2s. 5 20' 401 1,152 210 54 1,004 200 50 407405- 200 55 1,012 200 51 1 7 15 9. 1,010 207 61 5 When partsby welght of GR-S rubber are mixed with 58 parts by weight of the reclaims Spec fi v- 1-197 1-172 indicated at the heads of the column below and used respectively in a similar formulation and ABBASION tested, the following comparative results are ob- 1'3-5 tained: Loss, Loss, ccJHPH H ccJHIPH H Example 2 Example 3 Example 4 Natural GR-S Recaps 1,002 55 975 45 055 59 002 47 ,Cure

1" 035 60 942 48 69 Ten- T- gf Ten- T- "2 Ten- '1'. ggf

slle 300 on 5115 300 tion S 300 tion I 8) ll 7! I In Formulatlons B f C move the 50' at 451 2,000 820 505 2,000 550 510 1, 550v 530 525 lowing results were obtained: 45' at 4511 2,000 800 515 2,100 540 525 1,710 700 525 ,1 50 1 451 1,900 540 510 1,720 680 555 1,540 790 450 NATURAL COMPOUNDJORMULATION,,B,, o at 50# 1,450 720 450 1,050 550 550 1, 580 500 450 "Standard #5015? Example 7" 12101 'IENSILE (212 F.) Om T 131 H d 'r E1 H d E1 E1 E1 811- Oll- 81 611- OH- 81 5 011 27- On a- 0n 8- sile gation ness T 300 sile getion ness T 300 70 Tensile tier T811511 tio Tenslle do 30 at 280 F- 2, 548 500 55 91s 2, 501 520 55 895 50' at 45#. 745 350 555 550 535 555 45' at 280 F- 2,542 557 50 1,111 2, 757 570 55 1,059 45' at 45#, 755 540 545 330 520 515 50 51 220 F 2,545 507 51 1,215 2,557 525 50 1,154 50! at 451:" 570 500 450 250 520 505 7551 250 F- 2,557 500 52 1, 24s 2, 775 527 51 1,249 120' 51 50# 450 245 450 250 505 255 When 218 parts by .weightofthe reclaimbelow were used with 100 parts of natural rubber .the

following-results were obtained:

Example 2 Example? Example 4 Natural .GR-S Recaps Cure Ten- 'r- Ten- "r- Ten- 'rga- V ga,- g 5110 300 on sile 300 tion sile 300 on 30' at 45# 860 360 455 1, 480 260 '650 1, 310 380 600 45 at 45# 700 340 435 1, 340 280 600 l, 130 380 560 60 at 45# 660 300 440 880 .280 500 960 370 520 120 at 60# 500 240 450 480 280 390 560 360 430 nor rrENs1LEI 212 r.)

Tensile agi Tensile ggg Tensile i 30' at 45#.. 045 450 800 570 045 570 45 at 45# 470 400 "730 515 575 560 60 at 4 430 380 520 420 580 530 120 at 1 260 280 225. .260 180 550 FLEXOMETEB,

Example 2 Example 3. Example i Natural GR-S Recaps 60 at 45#. 17 17-45" 2630" 120 at 60#; 30 9' 17.30

TORSIONAL HYSTERESIS .Examplejz: Example 3. LE xample:4 Natural GETS. Recaps 30 at 45# 01088 0.081 0.084 45"at '4 .093 .080 083- 60 at 45;? .093v 109.0 0831 120 at 60# 106 126 .115

When 62.5 parts by weight of the standard" reclaim indicated above. .(near .the recital of Process 1) and the reclaims of Examples 2' and 3 are respectively mixed 'with .100 parts of GR-S rubber in a compound suitablefor tire side wall, and tested comparatively the following results are obtained:

T-300 r-aoo T-:a00

TORSIONAL HYsTEREsIs' Tests of Example 4 in comparison with Ex- 11:5 ample 3 in a similarly "proportioned compound give:

Example 4 with #1 "Example'li with Recap Stock Natural Rubber I Cure El n- Elon- Tensile 711300 Tensile T300 gation 'TORSIONAL HYSTEIRESIS 30 Example 4 Example 3 Using Formulation "C above. a GR-S compound, the .following. hysteresis-loss results are secured:

Standard Example 5 Cure Power- 'Inden- *Resili- Ilower. .Inrlen-. .Resili- Loss tation 'ence Loss .tation. .emce- '80at280 49.0 5.14 43.5 42.13 7.05 43.7 100at280 48. 4 2001 43.7 44.2 7.35 43.3 .120'.at.2s0F-. 110.3 7.180 43.9 12.9 7.18 43.4

The terms used lust above are explainediurther in detail just below:

Reference: The Vanderbilt 1942 Rubber Hand.- book, pages 291-299.

Definitions:

Resilience.The ratio of the energy of rebound to the energy Of fall. Indentation.Th penetration corresponding to the standard force value. The sum of the energy of fall and energy of rebound divided by the penetration isknown as the force value. The indentation is determined by plotting the penetrations against the force value for the various heights of drop and. reading the indentation onthe ordinate corresponding tothe standard force value point on the plotted curve, 7 Power loss-In the same manner energy loss that is the difierence between the energy plotted against .force value and the power loss read on the ordinate corresponding to the standard force value on the plotted curve. I

The produ t 015 the following p oc se of fall and the energy of rebound, is

also

exemplify the invention in certain of its aspects and give highly satisfactory results.

PROCESS 8 Using the following formulation:

Parts by weight No. 1 Peels natural rubber 24 mesh 95.00 .50 1.50

Tertiary dodecyl mercaptan Petroleum solvent (Solvesso No. 3) Engine oil Lecithin (clearate) Water In the machine of Fig. 2 at a worm speed of 48 R. P. M. the temperatures were as follows:

300 F. in the intake pipe l6 320 F. in the outlet pipe 22 350 F. rear 361 F. center 362 F. forward 150 F. at the rear of the cone 144 F. at the forward end of the cone 326 F. at the die (1. e. chamber 3|) The stock moved through at a rate of 49.4 pounds per hour with a power input of 10.5 horsepower and a transit time of 3.8 minutes for passage of stock along the length of the chamher 6.

Example 8 The product was a good quality reclaim with a specific gravity of 1.143 and a plasticity number of 4.70.

A product of Process 8 when cured gave the following physicals:

Cured with R.A;F.50% Tensile gg Hardness Abrasion (/0- E paper) cc./HPH

PROCESS 9 T J'sing the machine of Fig. 2 with extrusion- 253 F. oil inlet 273 F. oil outlet 279 F. rear 336 F. center 365 F. forward 350 F. at the die 174 F. at the forward end of the cone The stock was run through at a rate of 43.8 pounds per hour using 9.5 horsepower. The transit time for passage of stock from the feed end of the screw to the cooling chamber 2'! was 4.3 minutes.

22 Example 9 The product had a specific gravity of 1.122 and a plasticity number of 3.85.

A product of Process 9 when cured gave the following physicals:

Cure, RAF 70% T E H PROCESS 10 A mix such as described in Process 9 was processed similarly in the same machine, the temperatures being as follows:

345 F. oil inlet 350 F. oil outlet 357 F. rear 411 F. center 407 F. forward 365 F. die

155 F. forward cone and was run through at a rate of 52.5 pounds per hour at approximately 10 horsepower and a transit time of 3.5 minutes.

Example 10 Product of Process 10, having a specific gravity of 1.12 gave a Williams plasticity of 2.79 and a Mooney viscosity (ML/180/1.5/l) of 58. When cured at 40 pounds of steam in a 70% RAF for-" mula, a product of Process 10 gave the following physicals:

Elonga- Tensile Hard- Minutes tion,

pounds percent ness When cured fifteen minutes with 70% RAF a torsional hysteresis figure of 0.089 was obtained.

PROCESS 11 Ninety-five parts by weight of 30 mesh natural rubber #1 peels were mixed with 0.5 part of tertiary lauryl mercaptan, 1.5 parts of Solvesso #3, 1.5 parts of engine oil, 0.5 part of lecithin, and 1.5 parts of Water and run through the machine of Fig. 2 at a worm speed of R. P. M.

The temperatures were as follows:

301 F. oil inlet 316 F. oil outlet 351 F. rear 370 F. center 368 F. forward 152 F. rear cone 158 F. forward cone 318 F. die.

The stock moved through at 52.9 pounds per hour with a power input of 11.2 horsepower and a transit time of 3.5 minutes.

Example 11 The product was an excellent quality reclaim with a specific gravity of 1.143 and a plasticity number of 4.70.

A product of Process 11 gave a thermal softening factor of .516 derived from Mooney viscosity r1. .oil.0utlet. 151- 3,768 B. rear 399 F. forward 307 F. die

241 F. forward cone The stock was run through at a sgeedof i 2514. pounds per hour 13.? horsepwer,-.anda transiftime of '7 minutes.

Example 12 There was produced a flat. product. which. althonglrdry, and.hard,.had;very. desirable. pronerties. The specific gravity. was:- 1.478". andlth'e plasticity number 6.10.

A product of Process 12 when cured gave the to and is approximately long A die in followingphysicals-z.

R2.A.E;% n. 11-.

PROCESS 13 Using the machine of Fig. 2 with extrusion 386 ET. fhrward 5,

.17 F. die 204 F. forward cone The stock was run through at. a. rate. of- '73. pounds per hour and 15.1 horsepower. The transit time was 2.5 minutes. a specific gravity of 1.168 and a plasticity num=-- her when refined of 4.62.

Erample 13 Theproduct of Process, 13..

cur e, R. A. F. '1" i E: H

, PROCESS 14 Using. the. maohineeofj Fig. 2,- with. extrusion. 75,

into; air,. a. mix? similar? tothat; at. Procesm 13;.- except that thererwerednoluded, a1SD15 QaItStOf: Naftolen R-lOO, was. run, through with a cone clearance of 0.018 at a speed'of 45 pounds per hour at 12.6 horsepnwer: andiaxtransit'; time} of 4.1. minutes.

Example. 1 4

The product. had at specific: gravity of: andi a plasticity, number when: refined: ceases (ML/ 1 /,15/ l) viscosity, of. 6 6

The product had: 60

cmmsmrsm- '1 E5 a H1, figgs The quality factor is calculated as'follbws:

80994240 cease-7.5;"

PROCESSIS Using; a. shorter,, straightrline machine. with a.2'0" screwihavingae 1. 5" pitch. reduced. to. forcing, pitch.-atathelasttwoinches... The thread; is 5 d'eep forcing, 7""pl'asti'cating, and l 2" shallow forcing. The.cone.pin tapers from 3"" line with tlie -cone wasusedl afifi parts-of m mesh Bima S peels andi 49.5 par-ts of i 12 mesh. naturall rubber peels were mixed with 1 part of tertiary.

r7 la'uryl mercaptan; 1 .5 parts or Solvesso- No; 3

" and 0.5 part of lecithin and 1.5" parts of water and processed in theapparatus with a rotor speedof 70:12,; P..M.. The temperatures. were as follows::

279 F. oiLinlet;

295 F. oil outlets 342 F. rear 25131? forward cone 37191 die The stock: was run through at a rate of 221' pounds per hour at 9.2horsepower-and with; a. transit time a of. 8.4 .minutes.

Examzqle, 1.5.

The product on extrusion into air, yielded a goodl'lree'laimi with azspecifimgravity ofi'11L73z and aaplasticity numberof 42953 When cured (R'AF5U%-) it' gave: the follow ing physioals z lortibnai Hystere- PROCESS 16 In a procedure similar to thatnoffFro'cess 14'5 47.5 parts of 24 mesh natural rubberfp'eelfstandi 47.5 parts of Buna=S peels:weremixediwith lipart1 cone temperature of 220 F., and a die temperature of 270 F. The contact time was 9 minutes, and 11 horsepower input. A good reclaim with. a plasticity number of about 6.09 and a specific gravity of 1.150 was obtained.

Example 1 6 A product of Process 16, having a Mooney viscosity (ML/180/1.5-1-8) at the time of load testing of 106, assimilated 700 grams of Suprex clay per 500 grams of reclaim, on a 12" x 6" mill, and required a maximum of 4.08 horsepower while mixing in the last 100 grams of this amount, and a maximum of 3.86 horsepower when the load was all mixed in (4% of stearic acid was added on the clay). When this compound was vulcanized (1% of Zenite A, 1% of stearic acid, 3% of zinc oxide, and 3% of sulfur, had been added on an assumed RHC of 50%), for minutes at 307 F., the durometer reading was 89, the tensile strength was 443 p.s.i., and the elongation was 80%.

Cure, R. A. F. 50% '1 E H PROCESS 17 In a similar procedure a treatment generally similar to that of Process 16 was carried out with a contact time of 10 minutes, and an input of 12 horsepower hours, 0.5 part of lecithin and 0.2 part of 2-ethyl butyric acid employed in the mix, but no engine oil. Good results were achieved. Good results were likewise obtained using teritary lauryl mercaptan instead of the straight chain lauryl mercaptan.

Using a special machine, 95 parts of red inner tube scrap in crumb form of 12 mesh size were mixed with a solution consisting of 3.5 parts of Solvesso No. 3, 1 part of engine oil, and 2 parts of 'dioctyl' disulfide'. Ihe resulting mixture was passed through a tubing machine provided with a nozzle having an annular opening a few millimeters in radius and several inches in length electrically heated to bring the composition in the nozzle quickly to a temperature of about 400 F. and to hold it at approximately that temperature until discharged into an inert cooling bath or cooling atmosphere, by which the treatment was quickly terminated. The temperature of the mixture during passage through the nozzle was approximately 407 F. and the approximate transit time within the treating zone 3.1 minutes;

Example 18 PROCESS 19 The same mixture as in Process 18 excepting Example 19 The product was a reclaim of good quality with plasticity number 5.3.

Example 20 Using the following formulation;

Parts by weight No. 1 natural rubber peels (tire treads peeled from the carcass) ground to size adapted to pass a 24 mesh screen 95.00

Tertiary dodecyl mercaptan .50 Petroleum solvent (Solvesso No. 3) 1.50 Engine oil (Topsall No. 62) 1.50 Lecithin ,(Clearate), .50 Water ..1 1.50

' the mix was run thru the machine of Fig. 2 at a contact time of 2.91 minutes at 367 F; and a production rate of 62.0 pounds per hour with a worm speed of 60 R. P. M. This recla1m has a specific gravity of 1.122 and a Williams plasticity number of 4.73.

PROCESS 21 Prepared from a mix similar to the formulation in Example 20 except that the tertiary dodecyl mercaptan was increased to 5.0 parts by weight instead of 0.5 part and the engine oil was completely eliminated. This mix was processed in the machine of Fig. 2 for 1.46 minutes at 361 F. and a worm speed of 60 R. P. M., yielding a production rate of 123 pounds per hour.

Example 21 The reclaim has a sepcific gravity of 1.120 and a Williams plasticity number of 3.86.

A product of Process 21, having a Mooney viscosity, (ML/l/L5-l-1) at the time of load testing, of 54, assimilated 500 grams of Suprex clay per 500 grams of reclaim, on a 12" x 6" mill of 1:1.3 roll ratio, and required a maximum of 4.08 horsepower while mixing in the last grams of this amount, and, a maximum of 3.86

i T 1 1 sion oss ors one- T E H (SID-280 hysteresis paper) A thermal softening factor of .266 was obtained from Mooneys (ML//6/1-l'l) of 65.6 and (ML/212/6/1-17) of 5'7.

2 7 This reclaim h'as a quality factor calcfilated as follows:

763 XBI7 8 57 2X54 Examzile22 Prepared from a .mix similar to the formulation of Example 20 exceptthat 1.0 part by weight of imonomeric :styrene was added "-110 the :niix. This mix was then processeiiiinitheimachineaof Fig. 2 for 3.09 minutes at 358 F. with a worm speed of 60 R. P. M.,yielding a production rate of 58.2 pounds SDQIIhOU-l'. Ireclaim :has a specific. gravityof 1.121 and a Williams plasticity number'of 4219.

SERQCESSQfi sFormulation "No. 1 natural peels, 24mesh i ..1 95300 flerpinolene -1;.-25 Styrene monomer 1'00 Solvesso No. 3 1. Engine oil :1i50 Lem'fhin ...50 Water 1.50

Process-4215 minutes at"365 F..in the maliine of Fig. '2 at a worm speed of 60LR..P. M. "70

pounds per hour, Refined 0.003" maximum.

Example '23 The 'product 'of Process '23.

PROCESS .24

Formulation:

67% mixedbeadless tires V 6% 8-3 headless *1001'0 27%.70 graderpeels Tertiary dodecyl mercaptan .hp Petroleumresin' (PDO' 530 Petroleum asphalt. (Ne -.3186: res :0 Hydrocarbon solvent (Esso 200). 2.0

The above mix was "processed in the plasticator of Figure 2, at 69A pounds per hour, ;at.a .temperature of 303 F., :and a worm .speed ef :60 R.-P. M. V

,Emample 24 "Theproduct'of Process Ramp-A soft, tacky reclaim with=a William's plasticity "of 41 70 (3 minutes at -'7'0 0.) -and a Mooney viscosity XML/180715 1) :of --62.

Chemical analysis (partial):

"The load testing demonstrated that this *reclaim could-assimilate 600 grams 'ofsuprexclay per 500 grams of reclaim, "ona 12 x 6" laboratory rmill, havingra roll "speed ratio of 31:33 rflyanfi using 5104 horsepower awhile miixing iin the ila st 100.=grams:increment:'of this lead, and=4L8B;hO1SE- power when ztheil'oad'swa-s mixed in (4 o'f steam acid was added on thezclayi). fllhiszreclaimlcould assimilate 450 grams.of..a..semi-reinforcing furnace black (Furnex) per "500 grams of reclaim on the mill adeseribed above, *and' requiring 6.66 horsepower while mixing in the last '25 figs-am increment, and 51-71 horsepower when :mixed. This reclaim mas-equality factor, described by the=term:

Rens'ileX elongation Abrasion lossXMo'oneyviscosity as ffollows: '(Cure f30 Tmhiiites :28'7 T3 PROCESS 25 A mix composedzof 24-mesh-No. 1lrecappeelsnun ---.00 Tertiary .dodecyl mercaptanv1:00 .Lecithin. .i. No. 132 solvent 1.50 PRR No. 1 9.75

.was .processed .in ..the machine .offig. .3, operating .at 40 RIP. for .threeminutes at 141021 at .a rate @1300 .pounds iper hour and .refine'd :at 0.0035 inchmaximum.

.Examzile .25

.A product 'of'Bmcess25.

Analysis:

Acetone extr Total 5111 Free carbon- Cel1ulose -Ash Rubber; hydrocarbon (difierence) Rubber hydrocarbon (direct) Acidity (4 hr. boll) Specific'gravity r Evaluationliormula:

Smoked sheets seaa ase Thin pine far Sfpm'lc acid Sample Care at 260,F.

Modulus'300% .i

Tensile Elongation Soe'cifiegravity Reb. deli: (unaged):

.iRebound".

Deflexion. Regg flex! (66% 'unage Williams plast. (70 C.)

0-hours -1. 4-hours. :1O hour Abrasion" (Burean'ol' Standards Compression set (ASTMB)22 hours at 158 F 29 PROCESS 26 A mix composed of: 24 mesh GR-S whole tire scrap 95.00 Tertiary dodecyl mercaptan 1.00 PRR 14.00 Lecithin .50 Water 1.50 was processed in the machine of Fig. 3.

Ezrample 26 A product of Process 26. Analysis:

Acetone extract 21.36 Chloroform extract 4.87 Alcoholic KOI-I extract 1.03 Free sulfur .16 Combined sulfur 1.72 Total sulfur 1.88 Free carbon 20.89 Cellulose 1.60 Ash 6.93 Rubber hydrocarbon (difierence) 41.44 Rubber hydrocarbon (direct) 13.32 Acidity (4-hour boil) .013 Specific gravity 1.16

Evaluation formula:

Smoked sheets 38.00 Sulfur 4.30 Zinc oxide 5.45 EP channel black 19.65 Captax -1 .75 Thin pine tar 3.10 Stearic acid 3.00 Sample 113.00

Test 55 Orig. Aged 25 $92 1 S 8 Modulus 300% 188 1, 075 1: 550 25 i228 i522 Tensfle 13g 1: 775 11 775 25 238 $52 E on 38 435 345 Specific gravity l. 155 Rebound-defiexion (unaged):

Rebound 65 52.0 Deflexion 6 261 Reg flex. (66% ungged) 50 74 Williams plast. (7O 0.). 280 26 317-68 340-131 S t 56 257mm Comm set 50 6 52 69.2

, Whole tire.

PROCESS 27 7 3 1 1 lx ed tires 6 GR-S tires 70 grade peels (in which the natural rubber content is approx- ,mately 70% of the total hydrocarbon).

Tertiary dodecyl mercaptam. PDO4O defiberlzed and ground to 18 mesh 100 Ola BR E330 (coal tar hydrocarbon sp. g. 1.251.32)

The above mix was processed in a machine similar to the plasticator of Figure 2, having a feed screw of four times the diameter, and 4.5 times the length, at a rate of 1450 pounds per hour, and a Worm speed of 20 R. P. M. There:

3'0 sulting raw product was refined once through rolls set at .0035" maximum.

Example 27 erties were as follows:

Tensile Elongation i specificygrav' A product of Process 2'7, having a Mooney viscosity (ML/180/L5-1) at the time of load testing of 26 assimilated 700 grams of Suprex clay per 500 grams of reclaim, on a 12" x 6" mill, and required a maximum of 4.02 horsepower while mixing in the last grams of this amount, and a maximum of 3.81 horsepower when the load was all mixed in (4% of stearic acid was added on the clay). When this compound was vulcanized (1% of Zenite A, 1% of stearic acid, 3% of zinc oxide, and 3% of sulfur, had been added on an assumed RI-IC of 50%), for 10 minutes at 307 F., the durometer reading was 80, the tensile strength was 622 p. s. i.., and the elongation was l A product of Process 27, having Mooney viscosities (15 days) (Ml/180/1.5-1) of 27%;. (ML/180/3-1) 0f 23, (ML//6-1) of 21; and a Mooney viscosity (ML/212/1.5-1) of 21, (ML/ 212/3-1) of 18 2, (ML/212/6-1) of 1'7; and a Mooney viscosity (ML/244/L5-1) of 19, (ML/ 244/3-1 of 16 and (ML/244/6-1) of 15; and a Mooney viscosity (ML/l60/1.5-1) of 36 (ML/ /3-1) of 29 (ML/160/6-1) of 26. This product had a thermal softening factor of 0.25 between ML/160/ 6-1 and ML/ 61; a thermal softening factor of 0.13 between ML/ 180/ 6-1 and ML/212/6-1; a thermal softening factor of 0.062 between ML/212/6-1 and ML/244/6-1; and an overall thermal softening factor of 0.131 between ML/160/6-1 and ML/244/6-1.

PROCESS 28 Example 28 The final product was a smooth reclaim having a Williams plasticity number of 5.10, for 3 minutes at 70 C. This reclaim (specific gravity 1.137) when cured in the Reclaimers Association Formula for 50% rubber hydrocarbon for the times shown at 40 p. s. i. had the following physical properties:

Tensile ggg Hardness Abrasion 25 min. at 40 p. S. i 637 333 39 30 min. at 40 p. S. l 705 330 40 642 A product of Process 28, having a Mooney vis 'cosity (ML/160/L5-1) 0f 44%; (ML/160/3-1) of 35 (ML/160/6-1) of 30; and a Mooney viscosity ween e-ms (ML'lJiSOf-lfi-l) mi 332%, (ML/ 113M340 :of 21, and (ML/180/6-1) ofzlzst;randzaMooney viscosity (ML/'2l2/l.51) f 26, (ML/2l2/3l) of 22%, (ML/212/6-1) of /2; and a Mooney viscosity runny e 1) er ee /2. This :product had a "thermal softening factor of 0.1 1 between ML/ IEO/B- I) "and GVIL/ZI Z/B-D -*and a thermal softening factor of 01062 between I (MLI 21276-1) and (ML/ZM/G-l); and an over all thermal softening factor of 0.14 between (ML/lGO/G-l) iand-(ML-244/6-1-). 'The .quality factoris caliculated as follows:

immense 1-29 "100 parts or '12 ,mesh natural 'rubber clack inner tubes were :mixed with "015upart .of tertiary do'decyl mercaptan and '15 1 parts of petroleum solvent, and processed ata rate (if-350 pounds per hour inlthe machine oLFigure'B. The contact'time was 2:56 minutes, and theiten perature .was 353' F. "TheLresulting produchwasg'iven'a single refining at ".0035" maximum.

=-Eazampla29 A product of "Process 29, having Mooney "visco'sities (1 5 days) (ML/180K154) o'ff28, '.(ML/

Mooney viscosity (ML/212/1i5 1') of "23, (M147 212/3 1) "of 21,'and.(ML/21"2/6-.l) 70f "18. This product had a thermal :softenin'g factor of 1013 cific gravity,1.l42.

This ,product :hadithe following 1 physical properties 1 Kpprommatly-90%' ofthe 'rubberliydrocarbon'isnatural.

.The aboveinii-x was processe'diina machine similar to "the plasticatorloflFigurelibutlhaving a feed screw of "four times the diameter, "and 4.5 times the lengthgatsa'srate of 1250 pounds per hour, anda wormspeed .of .203. ,EwM. II'he resulting .raw product wasirefined once lthrough U rolls set :at 10035" maximum.

Emmzile =30 The efinished reclaim had a iwilliams plasticity of 3.34 for 3 minutes at 70 C. *Whenvcureddn the Rubber ReclaimersfiAssociation.Eormula -at 50% rubber hydrocarbon, and cured for 30 minutesat- IO p. s.zi. steam,the reclaim had the followingphysical properties:

i Elonga- Shore Specific Tensfle' 'tion "hardness gravity 30.min.-at -40 p; Si 1 824 i323 -42 2111 A product of ProcessffiD Lhaving a Mooney viscosities (8 days) (ML/180/r1.5- 1) of 26, ,(ML/ 180/3-1) of 21, (ML/l80/6-i1) .of 18; and a Mooney viscosity '(ML/212/1I5-A1) of 17, (ML/ 212 34) df10,'(ML/212/61) of14. "This prod- .uct'had a thermal softening factor of .0Jl3he- ,tween "MLY 18076-1 and 'ML/2I2/6 1.

Viihile there are given above certain specific examples of itliis' invention and its application in practical use and also certain modifications and alternatives, it should be understood that these are not intended to be exhaustive orto be limiting of the invention. "Onthe contrary, these illustrations and the explanations herein are given inmrderto acquaint "others skilled "in the art with'thisinvention 'and'therprinciplesthereof and a suitablemannerdfitsapplicationin prac- 'tical use, 'so that others skilled in the art may be fenabled to "modify the-inventionfand to adapt it "and applyit'innumerousforms, teach as may be best 'suitedto'therequirement of *a parti'cular use.

The term"vulcanized'rubber "as usedin the appended "claimsfis iritend e'dto 'inc'ludeipro'ducts :drived -from 'or -comprising natural 'or synthetic jdidlefin polymer "materials, ':butyl rubber, and mixtures thereof "with each "other, and/or "with other materials as commonly found ordealt with in the commercial rubber art.

Certain subject matter disclosedhutnot claimed .herein is claimed in certain of our copending applications as -follows: "381474, lliily 13, 121948; .l-QSJSGQ; November 2, I950; 19-3 088, November 2,1950; 293,25; December 29, I950; 233,445,:June :25, 1951; 246,327, September 112, 7:19.51; 346,328, :September 12 1951.

.The term fpolymeric as used in the -appended claims is to be understood in its generic sense as referring to co polymers-or inter-polymers (of Wh'ich GRHS -isan example), 'as well as to polymers -formed from -a single monomer (of :which natural rubberiis an example) and to mixitures and'combinations-thereof.

We claim:

1. A reclaimed material "formed 'from sulfur- *vulcanized rubbery hydrocarbon polymeric scrap, fat least'50% o'fathe monomeric units of theru'bbery hydrocarbon polymeric material 'therein being from the group consisting of butadi'eneiand isoprene, said ?reclaim retaining substantial amounts of combined sulfur of vulcanization, and :having a aspecific; gravity of not over "about 1.20,;and :a Mooney (ML/l80/12'5I) viscosity of from about. 32 toabout -'7-l *andzhavingawhemcured the Reclaimers Association Formula (50%) for 30 minutes at 287 F. a tensile strength of at leastabout 705 -p. s.- i., apercent-elongation of at least about 240, an abrasion loss (Oct/ 11E 13. h. 8/0-280 paper) ofrnotnver. about 642, and giving a quality factor defined as tensile strength percent elongation Mooney iCM'L/l80llj5el) visco.sity: .abrasioniloss 2; A reclaimed material as set forth in claim 1 which has a thermal softening factor one thirtysecond of the difference between the ML/ 180/6-1 Mooney viscosity and the ML/2l2/6-1 Mooney viscosity of not over about 0.37.

3. A reclaimed material as set forth in claim 1 which has a modulus of not over about 1000.

4. A reclaimed material as set forth in claim 1 which has a T-50 minus value which is no nearer zero than about minus 16.

5. A reclaimed material as set forth in claim 1 in the formation of which the chemical agent comprises an aliphatic mercaptan containing not less than 10 carbon atoms.

6. A reclaimed material as set forth in claim 5 wherein the mercaptan contains 12 carbon atoms.

7. A reclaimed material as set forth in claim 6 in the formation of which the chemical agent comprises monomeric styrene.

8. The process of plasticizing vulcanized rubber and like material which comprises progressively working the material in an extended form of thin cross-section under compacting pressure with substantial exclusion of air under conditions whereby heat generated by the working is accumulated to raise the temperature to not substantially less than 325 F., moving the material forward progressively while it is worked, maintaining the temperature between about 325 F. and 425 F., and progressively cooling the material at a succeeding stage in its progressive movement.

9. A process as set forth in claim 8 wherein the materia1 is comminuted prior to the progressive working, is mixed with ingredients adapted to facilitate plasticizing, and is extruded in thinner cross-section following the progressive working and forward movement thereof.

10. A process as set forth in claim 8 wherein the material is worked together with ingredients adapted to facilitate plasticizing, and wherein said progressive cooling takes place while air is substantially excluded.

11. A process as set forth in claim 8 wherein said progressive cooling takes place while air is substantially excluded, and wherein the material is further cooled thereafter by flowing a. stream of cooling fluid thereover.

12. A process as set forth in claim 8 wherein the material is worked together with ingredients adapted to facilitate plasticizing, and wherein the temperature is maintained between 380 F. and 410 F. during the progressive working.

13. In the method of extrusion in which a screw rotated within an extrusion cylinder is operative to cause heat-plasticizable material which is fed to the cylinder to be forced therethru and to be plasticized and worked during the course of its flow, such working of the material generating heat, the steps of progressively working the material in an extended form of thin cross-section under compacting pressure with substantial exclusion of air under conditions whereby heat generated by the working is accumulated to raise the temperature to not substantially less than 325 F., maintaining the temperature between about 325 F. and 425 F., adjusting the power input of said forcing and working actions to at least 0.1 horsepower hours per pound of material, cooling the worked material before discharge to reduce the temperature 34 .114. A process as set'forth'in claim 8 wherein the material is progressively worked in the presence of a reclaiming agent for a period of substantially one to twenty minutes.

15. A process as set forth in claim 8 wherein the material is comminuted and mixed with a chemical plasticization agent at a temperature not exceeding 250 F. before it is subjected to said. compactingpressure with exclusion of air.

16. In the method of extrusion in which a screw rotated within an extrusion cylinder is operative to cause heat-plasticizable material which is fed to the cylinder to be forced therethru and to be plasticized and worked during the course of its flow, such working of the material generating frictional heat, the steps of progressively working the material in an extended form of thin cross-section under compacting pressure with substantial exclusion of air under conditions whereby heat generated by the working is accumulated to raise the temperature to not substantially less than 325 F., maintaining the temperature between 325 F. and 425 F. for from two to ten minutes at a power input of from 0.15 to 0.83 horsepower hours per pound of material as the material is progressively moved forward and worked, and progressively extruding and cooling the material at the end of said working and forward movement.

17. A process as set forth in claim 8 wherein a plurality of different conjugated diolefine polymer materials are progressively worked together in the presence of at least one reclaiming agent.

18. A process as set forth in claim 8 wherein the material being progressively worked is repeatedly kneaded in the presence of a chemical plasticization agent.

19. A process as set forth in claim 8 wherein the material is progressively worked in the presence of a relatively small percentage of an aliphatic mercaptan.

20. A process as set forth in claim 8 wherein heat is externally applied to the material at an early stage of the process.

21. A process as set forth in claim 8 wherein the progressive working and forward movement involves an energy input of from about 0.15 to about 0.83 horsepower hours per pound of material, and wherein air is excluded during said progressive cooling.

22. A process as set forth in claim 8 wherein the temperature is maintained in range of from about 380 F. to about 410 F. for from two to three minutes.

23. A process as set forth in claim. 8 wherein the progressive working and forward movement is completed in less than three minutes.

24. A process as set forth in claim 18 wherein the chemical plasticization agent comprises monomeric styrene.

25. A reclaimed material as set forth in claim 1 wherein the rubbery hydrocarbon polymeric material comprises a copolymer.

26. A reclaimed material as set forth in claim 1 wherein the rubbery hydrocarbon polymeric material comprises a homopolymer.

27. A reclaimed material as set forth in claim 1 wherein the rubbery hydrocarbon polymeric material comprises a mixture of natural rubber and a butadiene-styrene copolymer.

JOSEPH C. ELGIN. EDWARD F. SVERDRUP.

(References on following page) 

1. A RECLAIMED MATERIAL FORMED FROM SULFURVULCANIZED RUBBERY HYDROCARBON POLYMERIC SCRAP, AT LEAST 50% OF THE MONOMERIC UNITS OF THE RUBBERY HYDROCARBON POLYMERIC MATERIAL THEREIN BEING FROM THE GROUP CONSISTING OF BUTADIENE AND ISOPRENE, SAID RECLAIM RETAINING SUBSTANTIAL AMOUNTS OF COMBINED SULFUR OF VULCANIZATION AND HAVING A SPECIFIC GRAVITY OF NOT OVER ABOUT 1.20, AND A MOONEY (ML/180/1.5-1) VISCOSITY OF FROM ABOUT 32 TO ABOUT 74 AND HAVING WHEN CURED IN THE RECLAIMERS'' ASSOCIATION FORMULA (50%) FOR 30 MINUTES AT 287* F. A TENSILE STRENGTH OF AT LEAST ABOUT 705 P.S.I., A PERCENT ELONGATION OF AT LEAST ABOUT 240, AN ABRASION LOSS (CC./H. P. H. 8/0-280 PAPER) OF NOT OVER ABOUT 642, AND GIVING A WYALITY FACTOR DEFINED AS 